Distilling method



June 23, 1953 Filed Dec. 5, 1946 J. LOUMIET ET LAVIGNE DISTILLING METHOD 6 Sheets-Sheet l IN VEN TOR. $16272 Loumz'e] efLaz/jgne June 23, 1953 J. LOUMIET ET LAVIGNE DISTILLING METHOD Filed Dec. 5, 1946 6 Sheets-Sheet 2 Fig. 2.

INVENTOR.

ATT RNEYS June 23, 1953 J. LOUMIET ET LAVIGNE 2,643,220

DISTILLING METHOD Filed Dec. 3, 1946 6 Sheets-Sheet 3 ATTORNEYS June 23, 1953 J. LOUMIET ET LAVIGNE DISTILLING METHOD 6 Shets-Sheet 5 Filed Dec. s, 1946 Q n m ATTORNEYS Patented June 23, 1953 DISTILLING METHOD Juan L'oumiet et Lavigne, Playade la Teja, Itabo, Cuba Application December a, 1946, serial No. 113,775

'In CubaDecember i, '1945 11 Claims.

This invention i-sin'the nature of an improvement upon my pending application Serial No. 6583508, filed March 30, 1946, for Distilling Process and Apparatus.

In that process the residues of any one of the operating columns were injected in the next column-of higher pressure so that the last one of those columns, namely, the column of highest pressure, accumulated all the residues of the feeding washes-tobe exhausted. That column of ili'ghes't pressure was then the only producer of ees.

Under such operating conditions all the water contained in the feeding washes was carried into the extreme column of highest pressure in this form of alcoholic liquid, partially exhausted, and the function of that column was to complete its exhaustion, extracting from it the alcohol it contains.

That final "exhaustion of the residues in the column of greatest pressure represents an excessive steam consumption. The present invention is directed to 'auoid that difiiculty.

If, .ior example, We :assume that the feeding washes contain alcohol and 95% water, 19 parts of water enter the apparatus with one part of alcohol. All that water is brought together in the column of highest pressure in the form of a poor 'alcoholi'cliquid destined'to be exhausted in that column.

But it is a 'fact that for obtaining that exhaustion it is necessary to consume at least 9.09 parts of steam per 100 parts of operated liquid.

In effect, the distillation of a liquid mixture of alcohol and Water does not produce a pure alcoholic vapor but a mixed vapor of alcohol and water containing a greater proportion of alcohol than the liquid. The vapor produced is in the best case, eleven times richer in alcohol than the liquid. Consequently, if a. is the amount of alcohol contained in 100 parts of liquid to be distilled, 11a would be the maximum amount of alcohol that could be contained in 100 parts of issued vapor, and that vapor would contain 100-imparts of water per 11c parts of alcohol issued from 1100 parts of liquid, that is,

per 100 parts of liquid.

The theoretical consumption of steam comprises. that 9.09-a and complementarily a consumption equal to approximately 0.40a to evaporate the amount a of alcohol, that is, in total 9.090.60a.. Considering that a is in its turn 2 very small, it could be assumed that the minimum :of steam consumption at the bottom of the column of highest pressure is 9.09% of the lees it produces.

To that expense must be added the consumption of the calender of the proper column which may be estimated at 3% of the same lees.

The'total minimum consumption woud be then about 12% of the lees, and since We have reckonedformerly 19 parts of lees to one part of alco'ho'l produced in the plant, the consumption of steam Water per part of alcohol produced would be an amount that is now considered excessive.

The present invention diminishes that consumption, providing that all or at least the greater part, of the successive columns, produce the final exhaustion of a part of the liquids they operate. In that form the water of the feeding washes is partially evacuated with the lees produced in all those exhausting columns, and therefore, only the rest of the same is operated in the form of poor alcoholic liquid in the column of highest pressure. If the water evacuated in that column is reduced to one-half or to 40% of the total water of the washes, the steam expense is re duced proportionately. The pointed out difficulty would be overcome and the amount of operated liquid in the column of highest pressure would be determined principally with the object of generating vapor enough to operate the columns of lower pressure.

If it is desired to raise the alcoholic richness of the product it is advantageous to obtain, par tially at least, rich condensates, and for this reason to fractionate the condensation opera-- tions.

The successive steps of a fractional condensation of a not very rich alcoholic vapor, are efiect'ed at successively decreasing temperatures with a possible interval of more than 20 F. and even greater. It is then advantageous to cause to heat with the heat made available in the first step of the condensation, the distilling operations efiected at a higher temperature, and with the heat yielded by the other successive steps, the other operations of the column effected at lower temperatures, the relationship being such that when the temperature of condensation of a step is less, the temperature of the distilling operation heated by that step .is also less.

'Onthe other hand, 'all along the height of the =2.28 parts a calender the alcoholic richness of the ascending vapor as well as that of the descending liquid increases successively from bottom to top, and consequently the temperature of the distillation decreases from bottom to top.

Hence is deduced the convenience of operating the steps of the fractionated condensation successively from bottom to top. In that form the temperature of the heating condensing fluid that run in the calender falls as soon as the temperature of the heated distilled fluid that runs in the tubes cluster falls.

Generally, the interval of temperature existing between the first and the last step of condensa- I tion of the heating vapor of the calender is much greater than the difference between the temperatures of distillation respectively at the lower and upper part of the tubular cluster. That consideration may lead to effecting in one column only the first steps of condensation of the heating vapors and to effecting the last steps of condensation of the remaining vapors in columns of smaller pressure and greater alcoholic richness.

The condensates produced in a column need not necessarily be employed in the same column as rectifying liquids. They may also find application in the following lower pressure columns not only as rectifying liquids but as supply liquids. They may also in certain cases find application to the column from which they issued, which represents the classic case of retrogradation. This standard retrogradation may be employed to a certain extent, because the conden-' sation of alcoholic vapors that heat a column fulfills two requirements which generally do not counterbalance one another; the need on the one hand of producing a sufficient quantity of heat for the distillation; and the need on the other hand of supplying a rectifying liquid which permits raising to the desired level the richness of the vapors of this distillation. The excess of calories which can produce condensation, utilizable for the second purpose, may often be usefully absorbed by the known process of partial retrogradation of the condensates of a portion of the vapor produced.

The supply for the low pressure columns is therefore partially furnished by the condensation from the preceding column operating at higher pressure. In the last one or more of these columns the supply may be composed exclusively of these condensates, and preferably of a plura1- ity of these condensates of different alcoholic richnesses which are injected into the column, each of them at the point where the treated liquid has an alcoholic richness equal to or less than its own. The other way around, a column may be interposed in the supply for the preceding higher pressure columns. For this purpose liquids that are more or less exhausted are extracted from this column and are injected by pumping into one or more preceding higher pressure columns, approximately at the points where the liquids being operated on in these columns have an equal or slightly higher alcoholic richness. 7

Most of the liquids supplying the alcohol columns contain calcium sulphate. In order to avoid incrustations of this salt, whose solubility decreases considerably as the temperature rises, the invention provides for superheating the supply liquid, prior to its introduction into a column, to a temperature sufficient to precipitate all the calcium sulphate that the residues of the column are unable to dissolve. This superheatwhich are applied to the purification of the operated liquids; a new rectifier of the vapor distilled in a column, and the appropriate modifications of the calenders of the distilling rectifying units described in my former application Serial No. 658,508, filed March 30, 1946, to adapt them to the fractional condensation.

In the annexed drawings, given by way of example:

Fig. 1 shows schematically the exhausting group of a general installation for the production of alcohol;

Fig. 2 shows a vertical section of a sedimentremoving reheater comprised in Fig. 1;

Fig. 3 shows a vertical section of a vapor protector, by the spontaneous evaporation of small amounts of water, which is comprised in Fig. 1;

Figs. 4 and 5 show in horizontal and vertical section respectively a fractionated condensation type distiller-rectifier comprised in Fig. 1;

Figs. 6, 7 and 8 show by'the first figure a ver-' tical section of the complete rectifier utilized in Fig. 1, and by the other two figures the details of one of its coils in horizontal and vertical section, respectively;

Fig. 9 is a flow sheet illustrating the flow of fluids in the apparatus.

In Fig. l is shown the exhausting group of a general installation for the production of alcohol, comprising fiv apparatuses or columns D, C, B, A operating at different and successively lower temperatures.

The wine that is to be distilled arrives at MA, and fiows' in succession through the sedimentremoving reheaters HA, 12A, 13A, MA, I5A, being pumped from one to the other by the pumps 33A,

34A, 35A, 36A. Upon emerging from ISA it is forced by the pump I3IB into the tube 66A, which divides and sends a. portion of the wine to column A through 12A, and sends the rest into the sediment-removing reheater [2B, This part of the wine is forced by pump 3lC, upon emerging from 1213, into the tube 66B, which divides. A portion of the wine that it carries is sent by tube 52B to the column B, and the rest is sent through tube 650 to the sediment-removing reheater [2G, and from there it passes to column C through tube 660.

A portion of the incompletely stripped wines from column A is also utilized for supplying the preceding columns B, C and D. This partially stripped wine is extracted from the intermediary reservoir 3-A of the distilling-rectifying unit of column A, and is forced by the pump Iii-B into the tube 'HB which carries it to the sedimentremoving reheater I IB.. It leaves this by the tube 12B, which branches before its entry into pump 1 36C. A portion of this wine is thus conducted wine to the dome of the distilling rectifying unit of column C. The rest of the wine is forced. by pump 3 ID to the dome of columnD. through the sediment-removing reheater [ID and the tubes 96D and 12D.

The column D has no rectifying. unit, and comprises only a distiller-rectifier of the type of Figs. 4 and 5. This apparatus is composed of a tubular cluster comprising the tubes I12 supported at their upper and lower ends by the plates I52 contained within a cylindrical casing I50. This casing is extended below the tubular cluster, forming a reservoir divided into two parts; the upper part where the tubes have their;

outlet and which evacuates their residual liquid through the tube I54; the other and lower part constituting a reservoir supplied by the tube I55 with vapor that it injects through the tubes. I56 into all the tubes of the cluster. One tube corresponds to each tube of the cluster.

The same casing is extended above the upper plate I52 in the form of a dome, comprising a, supply tube I58 which descends sufliciently low on the plate to form a hydraulic joint with the liquid that covers the plate. This tube is situated eccentrically relative to the dome, and the annular crown comprised between this tube and this dome is transformed into a separating coil for the liquids carried along by the vapor produced by the helicoidal surface I59.

The central casing is divided by approximately horizontal diaphragms I63 to I61 into five stages through which flows downward the vapor that condenses.

The vapor guided by the vertical diaphragms I62 fiows with a rotary movement through each stage from its periphery to its center, and inversely. In the stages in which the flow is from the center to the periphery, the condensations are collected in a gutter I64 situated at the outer edge of the diaphragms, and are evacuated by the tubes I65. The center of the diaphragm is open as shown at I66 to permit passage of the vapor from th lower stage to the higher stage.

In the stages in which the vapor fiow is from the periphery to the center the extraction of the condensates is effected by central tubes I70, I68 and I69 respectively. All these extraction tubes may be provided with automatic cleaners or with extraction regulators. The horizontal diaphragms have slopes, and the vertical diaphragms have numerous passageways to facilitate the movement of the condensates into all areas.

In the distilling-rectifying unit of column B,

which is heated by steam introduced through the tube ID, the extraction tubes are connected with one another and the. condensed water is carried to the boilers by the tube 8 ID.

The partially stripped liquids which supply it through the tube I58 (Fig. 4)v descend down the tubes of the tubular cluster, using up their alcohol through distillation and rectification, and reach the lower part totally stripped, constituting the lees of highest pressures. injected at the bottom of the column. through. the tube 8D. The mixed vapor of water and alcohol on the contrary rises along these tubes, increasing in volume and in richness. Before going out of the dome through the tube I60, it is purged of the liquids it carries with it by the separating centrifuge constituted by the annular space com.-

prised between the wall and the tube l58 trans-.

formed into a coil by the helicoidal. strip I59.

The mixed vapor of water and alcohol pro- Live steam is 6. duced at D is conducted through the tube 92D to the bottom of the casing of the distilling-rectifying unit of column. C. There it operates like steam in column C, and the collected condensates are sent through the tube BIC to the upper part of the rectifying unit of column B. However, the most volatile part of this vapor does not condense there, and is sent through tube 936 to the upper casing of the distilling-rectifying unit of column B.

Column C comprises a distilling-rectifying unit which is itself surrounded by a rectifying unit of the type of Figs. 6, 7 and 8. This rectifying unit operates in accordance with the process described in U. S. Patent No. 2,182,566 by single-stage operations comprising: injection of the rectifying liquid into the flow of vapor that is to be rectified, its atomization by this vapor, and the subsequent separation of the. vapor from the rectifying liquid it carries along with it.

The rectifying unit (see Fig. 6) comprises the annular space enclosed by the two cylinders Itl and I02 transformed into a coil by the helicoidal strip I03. 'Ihe vapor that is to be rectified flows downward through this coil. The cylinders NH and I02 are eccentric relatively to on another. Thi eccentricity produces great variations in the section through which the vapor passes. At the point where this section is a minimum (see Figs. '7 and 8) the passage is obstructed by a drum I I! which has openings provided with alternately converging and diverging tubes I06. At these points the section through which the vapor passes is almost entirely reduced to that of these tubes; and consequently because of this arrangement the vapor emerges from these tubes with great speed. The drum is supplied with rectifying liquid, which emerges from it in the direction in which the vapor moves and through a multitude of small perforations I05 in the corresponding wall its. In emerging from this wall the jets of expanding vapor collide with the thin jets of liquid and atomiz this liquid. This produces an intimate mixture of the two fluids.

The section through which the vapor passes then increases, and the vapor speed decreases. The particles of rectifying liquid precipitated against the outer wall are collected, either by a gutter I08 at the outer edge of the helicoidal surface I03 or by a skimmer I07 situated along the outer wall I02 which retains these drops and conducts them to the gutter I08. A metal coil H0 forming a spring bears against the outer Wall, acts as a cornice, and deflects toward the center of the gutter the drops descending along this wall. The post-rectification rectifying liquid collected in this form in the gutter i013 descends, contrary to the movement of the vapor, along this gutter to fall into the tube I09 which prolongs it a little before it in this return movement reaches the drum III. The tube then conducts the said rectifying liquid (see Fig. 6). along and below the outer edge of the helicoidal surface, to the injection drum of a coil at a lower level, where the rectifying liquid will be applied anew, in the manner described in the foregoing, to the rectification of a more impure vapor. The new coil where the liquid is applied should be at a sufficient distance from the higher coil to permit the pressure of the liquid in the injection drum to expel it at a sufiicient speed through its fine outlet openings. In the figure, this interval is three coils.

' The. higher coil of the helicoidal surface I03 constitutes a separator of the liquid carried by the vapor, and injection of the rectifying liquid does not take place there. The liquid that is collected there is conducted to the fourth. The rectifying liquid that comes from the outside is divided between the second and third higher coils.

The cylinder IIlI which constitutes the wall of the rectifying unit surrounds at a short distance the distilling-rectifying unit. The vapor produced in this latter descends through this space to enter the lower part of the rectifying column.

The distilling-rectifying unit of column C operates, as has been indicated, on partially stripped wines extracted from the central reservoir 3A of the distilling-rectifying unit of column A, after these wines have been reheated and had the sediment removed in the successive apparatus IE3 and IIC. It also operates on the residual liquids from its own rectifying unit, which are raised to the dome of this distilling-rectifying unit by pump 310 through the tube 860. The lees are evacuated from this unit through the tube MC. Live steam is injected at the bottom of said distilling rectifying unit through tube 8C.

In its turn the rectifying unit of this column 40 operates on the vapors produced in the distilling-rectifying unit, which as has been indicated descend in the space comprised between these two apparatus to enter the first one by its lower inlet. (In the figure this sleeve is schematically represented by the tube SIC.) The rectifying liquid, which here works against the flow, is the wine that is to be distilled and which has previously been reheated and had its sediment removed in the successive apparatus IIA, 12A, I3A, MA, ISA, I23 and I2C. It is conducted to the upper part of thi unit through the tube 660.

The rectified vapor emerges in its turn from this unit through the tube 92C, which conducts it to the lower part of the distilling-rectifying unit of column B.

However a portion of this vapor is branched through the tube 940 which conducts it to the enrichment column of the type described in my former application Serial No. 658,508, which is not represented in the figures nor described in the specification because the invention does not supply any improvement to the same. The enrichment column is indicated diagrammatically in Fig. 9. The more important relationships of the enrichment column F to the other columns are clearly indicated in Fig. 9.

The distilling-rectifying unit of column B is of the type shown in Figure 12 of my former application Serial No. 658,508 having its calender divided to effect fractionally the condensation of the heating vapor in the form shown in Figures and 6. It represents two flow units superimposed vertically and separated by the reservoir 3B. It is supplied at its upper part with wine which is previously reheated and has had its sediment removed in the successive apparatus IIA, IZA, I3A, I4A, ISA and I23, and the wine is conveyed to the dome of this unit by the tub 12B, and by the return liquids of its rectifying unit which are raised by the pump 1313 through the tube 86B. The lees produced emerge through 4 IB. Live steam is injected at the bottom of said distilling-rectifying unit through tube 8B The condensates from the lower casing come together and are injected into the rectifying unit of column A, a little above the middle of this unit, and the condensates of the upper casing:

come together and are injected into the upper part of the same unit. The uncondensed vapors are conducted to the casing IA through the tube 93B.

.The vapors produced by the distilling-rectifying unit descend through the sleeve which separates this unit from the rectifying unit 43 which surrounds it (represented in Fig. l by the tube 9 IB) and entersinto this second unit through its lower inlet. They are there rectified by the condensates from column C, and emerge from the upper part of this unit through the tube 92B which conducts them to the lower casing 2A of column A.

Column A is of the type of column B. It operates however with certain differences. The condensates from its lower casing 2A are divided into two groups: the first corresponding to the lower stage are sent through the tube 8 IA to one of the upper coils of the rectifying unit of the same column in order to be utilized there as rectifying liquids, and the others are sent through the tube 82A to the enrichment column. The condensates from the upper casing IA are collected in three groups and also remitted by the tubes 83A, 84A, 85A to the enrichment column at different levels as though they came from one stage higher in the group.

The uncondensed vapors in the casing IA are sent through the tube 93A to the upper casing of the enrichment column.

The distilling-rectifying unit of column A is supplied at its upper part with wine which, previously reheated and with its sediment removed in the successive apparatus IIA, IZA, I3A, I lA, ISA is injected into its dome through the tube 12A, and is supplied with the residual liquids of the distilling-rectifying unit of the enrichment column, which are conducted through the tube 42F, and with the residual liquid from its own rectifying unit which is raised by the pump 31A through the tube 86A. A portion of these liquids, partially stripped during their passage through the upper tubular cluster of easing IA, is extracted from the intermediary receiver 3A in order to supply the preceding columns. The rest descends through the tubular cluster of the casing 2A, where its stripping is completed and its lees are extracted through MA. Live steam is injected at the bottom of said distillating rectifying unit through tube 8A.

The vapors produced in this unit descend through the sleeve (represented in Fig. l by the tube 9IA) situated between the distilling-rectify ing unit and the rectifying unit 4A in order to enter the lower part of this latter unit, in the passage through which they are rectified in succession by the condensates produced in the casing 2B and conducted through the tube SIB, and by the condensates produced in the casing IB and conducted through the tube 823. The rectified vapors emerge from the unit through the tube 92A, which conducts them to the lower casing of the distilling-rectifying unit of the enrichment column. I

Fig. 2 shows the details of a reheater and sediment remover such as II A, IZA etc. The apparatus comprises a cylinder I I9 divided into stages by plates in the form of concentric conical frus tums I22 having generatrices slightly inclined relatively to the horizontal, starting from the cylinder H9, and ending at the interior in a flangededge. A central rotating shaft I20 passes through the bottom of the cylinder, through a stufiing box, and carries conical disks I2I, each of these conical disks corresponding to a conical frustum plate I22 and covering, at a slight vertical distance, all the central opening plus a margin. The upper part is transformed by a. helix into a circular coil through which the vapor flows in emerging, and where it is stripped of the liquid it carries with it.

The bottom of the apparatus constitutes a decanter. The separated sludge emerges through the tube I I8, and is collected in the tank I29 provided with an upperand a lower tap, by whichthe sludge may be removed at intervals.

The wine enters this apparatus through the upper tubing I3I which projects it against the first conical frustum. From there it rains ofi upon the first conical disk I2I. By virtue of their shock against this moving disk, which may be corrugated or grooved, the drops of wine bounce off and split up, filling this part of the cylinder with fine particles of Wine in movement. When they descend directly or along the walls, they finally drop upon the lower conical frustum plate I22, where they are again treated in the same way, and so on.

The vapor comes in through the lower tubing I26, and passes upward through the cylinder, entering each stage through the central opening of its lower conical frustum plate, passing between this plate and the corresponding conical plate which covers it, and reaching the peripheral part of the cylinder, and from, there it returns between the same conical disk and the conical frustum plate immediately above it to seek the central opening of this plate, and so on until it passes through the central opening of the last plate. From this opening it passes into the outlet coil, where it is stripped of the liquid it carries with it, and from there it passes to the iment removers is principally produced through the spontaneous evaporation of the lees.

The apparatus employed to produce this spontaneous evaporation is shown in Fig. 3.

It is constituted by a cylinder I42 comprising a central rotating shaft I36 Which passes through the bottom of the apparatus through a stuffing box and which receives its movement from the exterior. This shaft carries finely perforated spinner baskets I33. Between two successive spinners an annular conical frustum plate I34, of similar construction to the conical frustum plate of the apparatus of Fig. 2, receive the lee that have been flung by the higher spinner and pours them into the spinner immediately below. Each spinner thus divides the liquid it works on into fine jets which it flings against the walls where they are broken up and rebound toward the interior. This atomization to a great extent promotes the spontaneous evaporation of the lees produced by their excess of temperature relatively to the pressure of the vessel. These lees enter through the tubing I38, which pours them on to the upper plate, and they leave through the tubing I3I. The vapor that is produced goes out throught the tubing I39.

The production and the utilization of the vapor for superheating the wines is effected in Fig. 1 as follows:

The lees from column D are conducted through tube 42D into the evaporator 22D. The steam produced is compressed in the thermo-compressor (ID by the live steam coming from line i, conducted by the tube 76D. These two combined steams are conducted by the tube 55D to the reheater and sediment remover I ID where they are applied to superheating the wine. The uncondensed portion of these steams emerges from the reheater through the tube 5813 to combine with the steam conducted through the tube 556 and to act together in the reheaters of column C. This movement is regulated by a valve that is not illustrated in the figure.

The lees treated in the evaporator 22D are transmitted by the tube 43D to the evaporator 2 ID which operates at a lower pressure than 22D. The steam produced in this evaporator is conducted by the tube 5IC to the thermo-compressor 'iIC, where it is compressed by the live steam from line 1 brought in through tube 78C. These two mixed steams emerge from the thermo-compressor through the tube 550, and combine, as, has been said, with the excess steam from the reheater and sediment remover of the column in order to work in the reheaters and sediment removers IIC and 12C. The uncondensed steams in these reheaters combine upon emerging from these apparatus in the tube 560, and combine later on with steam conducted by tube 553 to work in the reheaters of column B, all these movements being regulated by corresponding valves.

The lees treated in the evaporator 2ID upon emerging from that apparatus through tube 330 combine with the lees emerging from the distilling-rectifying unit of column 0, and when combined are conducted to the evaporator 2IC. The steam produced in this evaporator is conducted by the tube 5I-B to the thermo-compressor 'HB Where it is compressed by the live steam, taken from line 1 by the tube 1613, into the tube 55B. These steams combine, as has been said with the excess steam from the reheaters of column C and are conducted to the reheaters I23 and I IB where they work; the uncondensed parts of the said steams combine in the tube 58B; and subsequently combine with steam brought in through tube 55A to work in the reheaters of column A; all these movements being regulated by corresponding valves.

The lees utilized in evaporator ZIC, which emerge from this apparatus through the tube 440,, and the lees which emerge from the distilling-rectifying unit of column B, when combined supply the evaporator 2 IB. The steam produced in this evaporator is conducted by the tube EIA into the thermo-compressor 1 1A, from which it is compressed into the tubing 55A by the live steam taken from line I, by the tube 16A, which combines with it. These combined steams, as has been said, combined with excess steam from the reheaters of column B and are applied to heating wine in the successive reheaters Hm, I 5A, ISA, IZA and IIA. The uncondensed products in IIA are pumped by the pump 3 IA.

Prior to their entry into the reheaters I iA, I3A, IZA, and I IA, these steams have added to them respectively steams produced in the evaporators 24A, 23A,'22A and 2IA. The first of these evaporators 24Axis supplied with the lees which have been previously treated in the evaporator 24B and which emerge from the said evaporator through the tube 43B combined with the residual lees-from the distilling-rectifying unit of column A, conducted by the tube 42A. The total of the lees from the column passes through thesuccessive evaporators 24A, 23A, 22A and ZIA; and

because these evaporators operate at successively decreasing pressures, they produce in each of them a certain quantity of steam which is applied, as has been said, to heating the reheaters MA, l3A, I2A and HA respectively. To this end the steam produced in 24A, conveyed through the tube 54A, is mixed with the steam issuing from the reheater 15A and the mixture is applied to heat the reheater MA; steam produced in 23A, conveyed through the tube 53A is mixed with steam issuing from the reheater MA and the mixture is applied to heat the reheater 13A; steam produced in 22A, conveyed through the tube 52A, is mixed with the steam issuing from the reheater 13A and the mixture is applied to heat the reheater IZA; and steam produced in ZIA, conveyed through tube 51A, is mixed with the steam issuing from the reheater 12A, and the mixture is applied to heat the reheater HA.

The described devices are capable of detail modifications, the particular case described having been given by way of example.

I claim:

1. In a distilling process designed to extract a definite fluid from a binary mixture that contains it, by means of successive operations effected in exhaustion apparatus having a plurality of exhausting zones, and a complementary enrichment column operating on the final vapor product of the exhaustion apparatus, in which exhaustion apparatus a first vapor injected or produced at the bottom of a zone is progressively enriched while the fluid operated upon, moving countercurrent to that vapor, is progressively exhausted, the final product vapor of said exhaustion apparatus being enriched in the complementary enrichment column which liquifies and separates from said product vapor a liquid residue containing the major part of the less volatile components mixed with a small part of the more volatile components, which residue is returned to the exhaustion apparatus; the improvement which consists in dividing the total current of original feed into a main stream and a plurality of secondary streams, in transmitting the main stream of original feed downward through successive zones of the exhausting apparatus, in each one of a plurality of those zones dividing a partial stream from said main stream, totally exhausting said partial stream, and removing its residue from the system; in exhausting partially in each exhausting zone but the last the remainder of the main stream and transmitting that remainder partially exhausted to the next following exhausting zone, in the last exhausting zone totally exhausting all the main stream operated upon and removing its residue from the system; in complementing each exhausting zone but the last, with a rectifying zone in which is enriched the vapor produced in the corresponding exhausting zone, in heating the final exhausting zone with steam; in passing the product vapors of each exhausting zone except the last into the corresponding rectifying zone to enrich them; in condensing the product vapor of the last exhausting zone and the enriched product vapors from each of the other exhausting zones except the first in indirect heat exchange with the liquid operated upon in the preceding exhausting zones in which vapors are produced; in feeding the first exhausting zone with the main stream of the original feed mixed with the residue of the enrichment column that operates upon the final vapor leaving the rectifying zone of the first exhausting zone and with the liquid residue of said rectifying zone; feeding each of the other exhausting zones except the last with the partially exhausted distillant from the bottom of the preceding exhausting zone, together with the liquid residue of its own rectifying zone; applying as rectifying liquids in each rectifying zone other than the last condensed enriched product vapor of a following zone, supplemented in at least one rectifying zone, other than the one that receives vapor from the first exhausting zone, by a secondary stream of the original feed total current.

2. An alcohol distilling process as described in claim 1, in which the various liquids that contribute to the feeding of a zone are injected in the operative units of that zone at different places according to their alcoholic contents, in order that the liquid injected at each point will be substantially the same in alcoholic content as that of the liquid already being operated upon at the same point.

3. A distilling process as set forth in claim 1 in which the condensation in a determined zone of the vapors produced in the following zones that contribute to its heating, is effected fractionally and the successive condensations extracted separately are applied at different places in the same zone and in anterior zones of lower pressure.

4. An alcoholic distilling process as set forth in claim 1 in which the liquids designed to feed each exhausting zone are previously superheated to a temperature higher by at least 15 F. than the temperature of the fluid operated upon in that step at the point of injection of said feeding, and sufficient to precipitate that part of the sulphate of calcium that would become insoluble during the operations of the step referred to, that superheating being effected by direct heat exchange with steam which is condensed, and said precipitate is removed from the liquid before the introduction of said liquid into the exhausting zone in which the step is performed.

5. An alcoholic distilling process as set forth in claim 1 in which the pre-superheating in liquid state of the liquid designed to be employed in a given zone is pro-superheated by direct contact with steam, produced by the spontaneous evaporation of the residual lees of the following exhausting zones of the same process.

6. An alcoholic distilling process as set forth in claim 1 in which the preheating of the liquid designed to feed an exhausting zone is preheated by direct contact with steam produced by the spontaneous evaporation of the residual lees of the following exhausting zone of the same process, compressed and amplified by live steam within a thermo-compressor.

7. A distilling process as set forth in claim 1 in which the rectifying liquid supplied in a zone is supplemented by condensations of the product of such zone in the amount necessary to absorb the excess of heat furnished by the condensation of vapor in such column.

8. In a process of exhausting an alcoholic binary mixture comprising several. steps, each step being performed in a distinct exhaustion zone at distinct pressure increasing from zone to zone as the exhaustion increases, with some of said zones operating at pressures higher than atmospheric pressure; a method for recovering the heat contained in the residual lees and applying said heat to steps of purification performed upon the liquids feeding said zones immediately before their admission to the successive exhaustion zones, which comprises: transforming the heat of the lees into latent heat of vaporization by successive flashes performed at successively decreasing pressures, and collecting in each flash the steam spontaneously developed to produce. and feed distinct streams of steam; utilizing each of said steam streams successively from the. first until the last to the previous heating by direct heat exchange of the liquids feeding the successive zones, respectively from the final zone of higher exhaustion until the first zone of lower exhaustion, and to that effect graduating the respective pressures of the successive flashes in order to provoke in each flash a temperaturefall of the lees flow appropriate to the temperature difference existing between adjacent exhaustion. zones; increasing the pressure and the flow of each stream by live steam within a thermo-compressor enough to respond to the requirements of a superheating at liquid state of the feeding liquids heated by said stream 15 F. at least above the temperature of the zone into which are injected at said points of injection; and removing from each such liquid the sediment produced'by said superheating prior to its feeding into the corresponding exhaustion zone.

97 A distilling process of a binary mixture effected in the exhausting column of a distilling apparatus which comprises anenrichment column of the final product vapors of said exhausting column, in which exhausting process the main stream of the original feed is progressively exhausted in successive exhaustion zones wherein the distilland flowing downward to the bottom is totally exhausted while in the first zones the main stream of that distilland is withdrawn partially exhausted at an intermediate level of the zone and directed to the following zones wherein is performed the exhaustion, which comprises: feeding mixed liquid to and causing the liquid to flow downward through a first exhaustion zone; withdrawing the main stream of the distilland at an intermediate level of said zone and feeding that distilland at an intermediate level of the second exhaustion zone and causing the liquid to flow downward until the bottom of said second exhaustion zone; causing the remainder of said distilland to flow downward through the rest of the first zone wherein it is totally exhausted and removing it from the system; feeding an original feed to the second zone and causing the liquid to flow downward through said zone; withdrawing the distilland at the bottom of the second zone and removing it from the system; supplying steam at the bottom of said second exhaustion zone for the purpose of heating; withdrawing vapors from the second exhaustion zone, at the top of said zone; condensing those product vapors in indirect heat exchange with the liquid operated upon in the first zone to produce vapors in said zone; withdrawing vapors at the top of the first zone, passing those product vapors in an enrichment column added to the first zone and withdrawing those enriched product vapors in an enrichment column added to the first zone and withdrawing those enriched product vapors of the first zone and directing the same to the enrichment column of the whole distilling apparatus as final product of the exhausting column; feeding the condensed product vapor of the second zone as rectifying liquid into the enrichment column of the first zone; and mixing the final reflux of said enrichment column with the final reflux of the enrichment column of first exhaustion zone and an original feed to provide an enriched mixed liquid which is the liquid fed to the first exhaustion zone.

lid

10. A distilling process of a binary mixture eifected in. the exhausting column. of a distilling apparatus which comprises an enrichment column of the final product vapors of said exhausting column; in which exhausting process the main stream of the original feed is progressively exhausted in. successive. exhaustion zones wherein the distilland flowing downward to the bottom is totally exhausted while in the first zones the main stream of that distalland is withdrawn partially exhausted at an intermediate level of the zone and directed to the following zones wherein is performed its exhaustion, which comprises: feeding mixed liquid to and causing the liquid to flow downward through a first exhaustion zone; withdrawing the main stream of the distilland at an intermediate level of said zone and directing the same to the following zones; withdrawing the. rest of the distilland at the bottom of said first. exhaustion zone and removing it from the system; feeding mixed liquid to and causing the liquid to now downward through a second exhaustion zone; feeding a portion of the distilland withdrawn at intermediate level from the first zone to an intermediate level of the second zone wherein it is mixed with the liquid flowing downwardv along said zone; withdrawing the. distilland at the bottom of the second zone and removing it from the system; feeding a mixed liquid to and causing the liquid to flow downward through a third exhaustion zone; withdrawing the distilland at the bottom of said zone and removing it from the system; supplying steam at the bottom of the third exhaustion zone for the purpose of heating; withdrawing vapors from the third exhaust-ion zone at its top; passing those product vapors in an enrichment column added to the third zone; condensing said enriched product vapors in indirect heat exchange with the liquid operated upon in the second zone to produce vapors in said zone; withdrawing vapors at the top of the second exhaustion zone; passing those product vapors in an enrichment column added to the second zone; condensing said enriched product vapors in indirect heat with the liquid operated upon in the first zone to produce vapors in said zone; withdrawing vapors at. the top of the first exhaustion zone; passing those product vapors intoan enrichment column added to the first zone and directing the same to the enrichment column of the whole distilling apparatus as final product of the exhausting column; mixing the remainder of the distilland withdrawn from the first zone at the. intermediate point with the reflux of the enrichment column of the third zone to provide the mixed liquid used for feeding said zone; mixing an original feed entering the system with the reflux of the enrichment column of the second zone to provide the mixed liquid used for feeding said. zone at its top; mixing an original feed entering the system with the reflux of the enrichment column of the first zone and with the reflux proceeding from the enrichment col umn of the whole distilling apparatus to provide the mixed liquid used for feeding the first zone; feeding an original feed entering the system as rectifying liquid of the enrichment column of the third zone; feeding the condensed enriched product vapors of the third zone as rectifying liquid into the enrichment column of the second zone; and feeding the condensed enriched product vapors of the second zone as rectifying liquid into the enrichment column of the first zone.

11. A distilling process of a binary mixture effected in the exhausting column of a distilling apparatus which comprises an enrichment column of the final product vapors of said exhausting column, in which exhausting process the main stream of the original feed is progressively exhausted in successive exhaustion zones wherein the distilland flowing downward until the bottom is totally exhausted while in the first zone the main stream of that distilland is withdrawn partiall exhausted at an intermediate level of the zone and directed to the following zones wherein is performed its exhaustion, which comprises: feeding mixed liquid to and causing the liquid to flow downward through a first exhaustion zone; withdrawing the main stream of the distilland at an intermediate level of said zone and directing the same to the following zones; withdrawing the rest of the distilland at the bottom of said first exhaustion zone and removing it from the system; feeding mixed liquid to and causing the liquid to flow downward through a second exhaustion zone; feeding a first portion of the distilland withdrawn at intermediate level from the first zone at an intermediate level into the second zone wherein it is mixed with the liquid flowing downward along said zone; withdrawing the distilland at the bottom of the second zone and removing it from the system; feeding a mixed liquid to and causing the liquid to fiow downward through a third exhaustion zone; withdrawing the distilland at the bottom of said zone and removing it from the system; feeding a second portion of the distilland withdrawn at an intermediate level from the first zone into a fourth exhaustion zone and causing the liquid to flow downward along said zone; withdrawing the distilland at the bottom of said zone and removing it from the system; supplying steam at the bottom of the fourth exhaustion zone for the purpose of heating; withdrawing vapors at the top of the fourth zone, condensing said product vapors in indirect heat exchange with the liquid operated upon in the third exhaustion zone to produce vapors in said zone; withdrawing vapors at the top of the third exhaustion zone; passing those product vapors into an enrichment column added to the third zone; condensing the major part of said enriched product vapors in indirect heat exchange with the liquid operated upon in the second exhaustion zone to produce vapors in said zone and directing the remainder of said product vapors to the enrichment column of the whole apparatus; withdrawing vapors at the top of the second exhaustion zone; passing those product vapors into an enrichment column added to said second zone; condensing said enriched product vapors of the second exhaustion zone in indirect heat exchange with the liquid operated upon in the first exhaustion zone to produce vapors in said zone; withdrawing vapors at the top of the first exhaustion zone; passing those product vapors into an enrichment column added to the first exhaustion zone and directing the same to the enrichment column of the whole distilling apparatus as final product of the exhausting column; mixing the 16 remainder of the distilland withdrawn from the first exhaustion zone at the intermediate point with the reflux of the enrichment column of the third exhaustion zone to provide the mixed liquid used for feeding said zone; mixing an original feed entering the system with the reflux of the enrichment column of the second exhaustion zone to provide the mixed liquid used for feeding said zone at its top; mixing an original feed entering the system with the reflux of the enrichment column of the first exhaustion zone and with the reflux proceeding from the enrichment column of the whole distilling apparatus to provide the mixed liquid used for feeding said first zone; feeding an original feed entering the system as rectifying liquid into the enrichment column of the third zone; feeding the condensed product vapors of the first exhaustion zone as rectifying liquid into the enrichment column of the second exhaustion zone; feeding different condensed enriched product vapors of the third zone at distinct levels according to the respective degrees of concentration as rectifying liquids into the enrichment column of the first exhaustion zone, and directing the condensed enriched product vapors of the second exhaustion zone to the enrichment column of the whole distilling apparatus for application as rectifying liquid in said enrichment column.

JUAN LOUMIET ET LAV'IGNE.

References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 643,702 Waterhouse Feb. 20, 1900 887,793 Guillaume May 19, 1908 1,136,559 Slavicek Apr, 20, 1915 1,145,728 Wiegand July 6, 1915 1,292,676 Barbet Jan. 28, 1919 1,587,188 Schneible June 1, 1926 1,957,818 Carney Mar. 8, 1934 2,048,888 Ott July 28, 1936 2,126,974 Reich Aug. 16, 1938 2,152,164 Wentworth Mar. 28, 1939 2,235,593 Schneider Mar. 18, 1941 2,289,191 Hall July 7, 1942 2,290,442 Metzl July 21, 1942 2,312,474 Peebles Mar. 2, 1943 2,327,993 Bragg Aug. 31, 1943 2,359,860 Kiefer et a1 Oct. 10, 1944 2,315,190 Eberhardt Mar. 30, 1945 FOREIGN PATENTS Number Country Date 182,711 Switzerland Feb. 29, 1936 OTHER REFERENCES Vapor re-use process, Othmer, Ind. and Eng. Chem, December 1936, pages 1435-1438.

Perry, Chemical Engineers Handbook, 2nd edition. McGraw-I-Iill, 1941, pages 1407 to 1412. 

1. IN A DISTILLING PROCESS DESIGNED TO EXTRACT A DEFINITE FLUID FROM A BINARY MIXTURE THAT CONTAINS IT, BY MEANS OF SUCCESSIVE OPERATIONS EFFECTED IN EXHAUSTION APPARATUS HAVING A PLURALITY OF EXEXHAUSTING ZONES, AND A COMPLEMENTARY ENRICHMENT COLUMN OPERATING ON THE FINAL VAPOR PRODUCT OF THE EXHAUSTION APPARATUS, IN WHICH EXHAUSTION APPARATUS A FIRST VAPOR INJECTED OR PRODUCED AT THE BOTTOM OF A ZONE IS PROGRESSIVELY ENRICHED WHILE THE FLUID OPERATED UPON, MOVING COUNTERCURRENT TO THAT VAPOR, IS PROGRESSIVELY EXHAUSTED, THE FINAL PRODUCT VAPOR OF SAID EXHAUSTION APPARATUS BEING ENRICHED IN THE COMPLEMENTARY ENRICHMENT COLUMN WHICH LIQUIFIES AND SEPARATES FROM SAID PRODUCT VAPOR A LIQUID RESIDUE CONTAINING THE MAJOR PART OF THE LESS VOLATILE COMPONENTS MIXED WITH A SMALL PART OF THE MORE VOLATILE COMPONENTS, WHICH RESIDUE IS RETURNED TO THE EXHAUSTION APPARATUS; THE IMPROVEMENT WHICH CONSISTS IN DIVIDING THE TOTAL CURRENT OF ORIGINAL FEED INTO A MAIN STREAM AND A PLURALITY OF SECONDARY STREAMS, IN TRANSMITTING THE MAIN STREAM OF ORIGINAL FEED DOWNWARD THROUGH SUCCESSIVE ZONES OF THE EXHAUSTING APPARATUS, IN EACH ONE OF A PLURALITY OF THOSE ZONES DIVIDING A PARTIAL STREAM FROM SAID MAIN STREAM, TOTALLY EXHAUSTING SAID PARTIAL STREAM, AND REMOVING ITS RESIDUE FROM THE SYSTEM; IN EXHAUSTING PARTIALLY IN EACH EXHAUSTING ZONE BUT THE LAST REMAINDER OF THE MAIN STREAM AND TRANSMITTING THAT REMAINDER PARTIALLY EXHAUSTED TO THE NEXT FOLLOWING EXHAUSTING ZONE, IN THE LAST EXHAUSTING ZONE TOTALLY EXHAUSTING ALL THE MAIN STREAM OPERATED UPON AND REMOVING ITS RESIDUE FROM THE SYSTEM; IN COMPLEMENTING EACH EXHAUSTING ZONE BUT THE LAST, WITH A RECTIFYING ZONE IN WHICH IS ENRICHED THE VAPOR PRODUCED IN THE CORRESPONDING EXHAUSTING ZONE, IN HEATING THE FINAL EXHAUSTING ZONE WITH STEAM; IN PASSING THE PRODUCT VAPORS OF EACH EXHAUSTING ZONE EXCEPT THE LAST INTO THE CORRESPONDING RECTIFYING ZONE TO ENRICH THEM; IN CONDENSING THE PRODUCT VAPOR OF THE LAST EXHAUSTING ZONE AND THE ENRICHED PRODUCT VAPORS FROM EACH OF THE OTHER EXHAUSTING ZONES EXCEPT THE FIRST IN INDIRECT HEAT EXCHANGE WITH THE LIQUID OPERATED UPON IN THE PRECEDING EXHAUSTING ZONES IN WHICH VAPORS ARE PRODUCED; IN FEEDING THE FIRST EXHAUSTING ZONE WITH THE MAIN STREAM OF THE ORIGINAL FEED MIXED WITH THE RESIDUE OF THE ENRICHMENT COLUMN THAT OPERATES UPON THE FINAL VAPOR LEAVING THE RECTIFYING ZONE OF THE FIRST EXHAUSTING ZONE AND WITH THE LIQUID RESIDUE OF SAID RECTIFYING ZONE; FEEDING EACH OF THE OTHER EXHAUSTING ZONE EXCEPT THE LAST WITH THE PARTIALLY EXHAUSTED DISTILLANT FROM THE BOTTOM OF THE PRECEDING EXHAUSTING ZONE, TOGETHER WITH THE LIQUID RESIDUE OF ITS OWN RECTIFYING ZONE; APPLYING AS RECTIFYING LIQUIDS IN EACH RECTIFYING ZONE OTHER THAN THE LAST CONDENSED ENRICHED PRODUCT VAPOR OF A FOLLOWING ZONE, SUPPLEMENTED IN AT LEAST ONE RECTIFYING ZONE, OTHER THAN THE ONE THAT RECEIVES VAPOR FROM THE FIRST EXHAUSTING ZONE, BY A SECONDARY STREAM OF THE ORIGINAL FEED TOTAL CURRENT. 